Process of synthesizing titanium-nitrogen compounds



" portions by-weight as follows:

' SKY and JOHN specification. 1 O

UNITED STATE S PATENT OFFICE.-

room) vou nIonowsxY Ann onN F.1IAR'1HAN, or Pomona, CALIFORNIA.

:rrtocnss or SYNTHESIZING' TITANIUM-NITROGEN 'co'mrounns;

80 Drawing. Application nled June .1,

T021llwk0mitmayc ncern: Be it'known that we, F 00131) VON Brorrow- F. HAn'rHAN, both citizens of the United States, residing at Pomona, in the county of ,Los Angeles and State of California, have invented a new and useful Process of synthesizing Titanium-Nitrogen Compounds, o'fwhich the following is a This invention relates .to the synthetic production of titanium-nitrogen compounds (under whichxterm we include the nitrid, and the, so-called, cyanonitrid, Ti( CN) .3Ti N by the reaction witha suitable titanium compound of nitrogen gas or a-mixture of nitrogen and hydrogen or ammonia gas. a

It is known, that nitrogen gas, either alone or in a mixtureof various gases, will combine with suitable compounds of titanium at a lower temperature and more rapidly, when the combining is etfected'in thepresence .of certain catalytically reactive agents, th& il ifthe catalyzer is not present.

min the process is composed of a mixture 1 containing an alkaline substance, a suitable group such,

titanium com ound, and a metal of the iron f er example, as iron, nickel, or

cobalt. The metal is employed to accelerate and lower the temperature of the reaction. The reactive mass also contains a re du'cing agent in the form of carbon." We at resent consider that the best form of cataytic reactive mass comprises a mixtureof .sodium carbonate, titanium dioxid, carbon,

- and iron, the iron preferably being in the 'finely divided metallic condition.

The components of the catalytic reactive mass may be combined, for example, 1n pro- Titanium dioxid 40 parts Sodium carbonate 10. parts Lampblack 10 :parts Iron filings 40 parts e catalytic reactive mass employed by.

. it possible to carry out the I moved, the remaining mass is I Specification of Letters Patent. Patented Sept, 192 1.

1920. Serial No. 385,561.

agent briquet form is then placed in up right or inclined retorts and heated to, a temperature of l000 While the reactive mass is slow current of nitrogen gas is passedtherethrough, the nitrogen gas ,being under a slight pressure, for example, twelve inches of water. When the mass reaches a temthus heating a perature of approximately 900 (3., the absorption of the nitrogen begins and the practical maximum of absorption of the nitrogen takes place at about 1090" C., or at a temperature just below that at which the iron, which has become saturated with carbon, melts, Were the temperature of the more or less.

catalytic mass increasedsufliciently to melt the iron, the iron would clog up the interstices in the mass and thus stop the flow of nitrogen'gas.

As exemplifying the; catalytic effect of the iron in the reaction, it may be'mentionedthat titanium dioxid and carbon without the other components of the reactive mass react but slowly at temperatures ranging from about 1400 C. to 1500 C; If sodium carbonate be added'to the titanium dioxid and carbon, the reaction proceeds more smoothly at a temperature of. about 1200 C. With the addition of iron, however, to. the other components,

the temperature may be reduced by at, least I reaction in tubes nilade of wrought iron, mild steel or special a o s.

T e heating of the catalytic mass is con tinued until the .nitrogen gas ceases to be tube in which the rereadily absorbed. The action takes place, having the space unoccupied by the reactive mass filled with nitrogen gas, is then allowed to'cool, the reaction mass 1s removed and broken up and the excess of iron is removed from the mass 111 any suitable manner as, for example, by magnetic excess iron; 1s rev attraction. After the washed with dilute acid. The resulting residue is then washed and dried and is treated with soda lime in a furnace to-re'move the nitrogen inv the form of ammonia, this operation being 200 0., thus making similar to the well known procedure of 'Verrantrap and Will for the estimation of nitrogen as ammonia;

be caused to combine steam at a dull red heat, or at a temperature ofabout 700 (7., which results in the obtaining of ammonia and hydrocyanic or the nitrogen may with superheated synthesizing titaniuming an oxygen-containing titanium comnitrogen compounds,

2o ing to a temperature ofnotover 1,100 C.

pound, carbon, an alkali metal salt and a' presence of metal of the iron group in the nitro an to form a nitrid.

2 e process for synthesizing titanium: nitrogen compounds, which consists in heating to a temperature of not over 1,100 C.

a mixture containing an oxygen-containing titanium compound, carbon, an alkali metal salt and a'metal of the iron group. in the presence of nitrogen gasto' form a'nitrid.

3.. The process for which consists in heat- The ammonia. then be freed which consists in heat-' synthesizing titanium- 1 a mixture containingf'titanium dioxid, so- 1 nitrogen compounds, which consists 1n 'dium carbonate, carbonvand particles of a heating an oxygen-containing titanium com- 7 an alkali metal salt anda metal ofthe irongroup in the presence of nitrogen under approximately atmospheric ressure at a temperature of about-1000 whereby impure mixtures of titanium nimid and. titanium cyanonitrid are formed. Signed at Los Angeles, California, this 24dayofMii1y1920. v OORDYON BIOHOWSKY.

JOHNEHARTHAN. Witnesses: I Gnonen H. Hmns,

' L. BELLE 'WEAvnR.

pound, carbon, 

